Separation and Purification Technology ( IF 8.1 ) Pub Date : 2022-07-30 , DOI: 10.1016/j.seppur.2022.121843 Lu Liu , Sinan Lu , Haiyan Liu , Ligai Bai
Stemonae Radix shows multiple pharmacological effects, mainly due to the alkaloid of tuberostemonine contained in it. An online SPE-HPLC method was fabricated by combining the solid-phase extraction (SPE) cartridge with a C18 analytical column through high-performance liquid chromatography (HPLC) system, which was used for the quantitative determination of tuberostemonine from Stemonae Radix extract and plasma. The SPE cartridge shows excellent matrix removal ability and specific selectivity for the tuberostemonine. The methodology validation confirms its good accuracy with the spiked recovery of 100.6%∼101.7%, a good repeatability with the relative standard deviations of 0.3%∼0.7% (tR) and 5.8%∼7.7% (A). Furthermore, the proposed monolithic SPE cartridge was used for the preparative separation and purification of tuberostemonine from Stemonae Radix, which was carried out on a semi-preparative HPLC instrument, with a high yield of 1.08 mg g−1 obtained. These results show that the present monolithic cartridge is an outstanding SPE adsorbent for the extraction, separation, enrichment and purification of tuberostemonine from Stemonae Radix, which can be extended to the analysis of similar alkaloids from complex samples.
中文翻译:
一种使用基于酰胺基的整体式小柱从百部中提取和纯化块茎甾酮的简单有效方法
百部具有多种药理作用,主要是由于其中所含的马铃薯碱生物碱。将固相萃取(SPE)小柱与C18分析柱通过高效液相色谱(HPLC)系统相结合,构建了在线SPE-HPLC方法,用于测定百部提取物和血浆中块茎甾酮的含量。 . SPE 小柱对马铃薯胺具有出色的基质去除能力和特定选择性。方法学验证证实了其良好的准确性,加标回收率为 100.6%~101.7%,重复性良好,相对标准偏差为 0.3%~0.7% ( t R ) 和 5.8%~7.7% ( A)。此外,所提出的整体式 SPE 小柱用于从百部中分离纯化马铃薯碱,在半制备型 HPLC 仪器上进行,获得 1.08 mg g -1的高产率。这些结果表明,该整体式小柱是一种出色的 SPE 吸附剂,可用于从百部中提取、分离、富集和纯化马铃薯碱,可扩展到分析复杂样品中的类似生物碱。